Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015) D3071

0013-4651/2015/162(11)/D3071/6/$33.00 © The Electrochemical Society

JES FOCUS ISSUE ON ELECTROPHORETIC DEPOSITION

Electrophoretically Deposited Polymeric Films: Evidence of
Correlation between Electrochemical Impedance Spectroscopy
Measurements and Morphological Properties
M. F. De Riccardis,z D. Carbone, and L. Capodieci
ENEA - Italian National Agency for New Technologies, Energy and Sustainable Economic Development, Technical
Unit for Materials Technologies, Brindisi Research Centre (UTTMATB), Brindisi 72100, Italy

Electrochemical Impedance Spectroscopy (EIS) was used in order to investigate coatings obtained by Electrophoretic Deposition
(EPD) from a morphological point of view. The analyzed samples were made of polyetheretherketone (PEEK), also mixed with
alumina or polytetrafluoroethylene (PTFE), and were characterized by different thickness, porosity and roughness. For each kind
of samples, a suitable equivalent circuit was used to interpolate EIS spectra. A linear correlation between thickness and Rcoat of
PEEK coatings was found, whereas an exponential correlation between Cdl and thickness and porosity was observed for PEEK-
Alumina composite coatings. Moreover, when the coating roughness was the most relevant feature, a Warburg element (with an
impedance equal to ZCPE = A/(jω)n ) was inserted in the equivalent circuit. In this case, the roughness was inversely correlated with
n. These results indicate that electrochemical impedance spectroscopy can be used as a non-destructive technique to evaluate, at least
qualitatively, the main morphological characteristics of EPD coatings.
© 2015 The Electrochemical Society. [DOI: 10.1149/2.0201511jes] All rights reserved.

Manuscript submitted June 3, 2015; revised manuscript received July 23, 2015. Published August 12, 2015. This paper is part of the
JES Focus Issue on Electrophoretic Deposition.

Electrophoretic Deposition (EPD) is one of the most outstanding
coating techniques based on electrodeposition. It consists in a first step
where charged particles, suspended in a liquid medium, move toward
the oppositely charged electrode under the effect of an externally ap-
plied electric field (electrophoresis). In the second step, the particles
deposit on the electrode and form a film whose characteristics, such
as thickness, porosity, and roughness, depend on process conditions
(concentration of particles in solution, applied electric field, time).1,2
The substrate acts as an electrode and the deposit of particles is the
coating. Sometimes a thermal treatment post-deposition is needed in
order to improve the adhesion to substrate or the coating density.3
Usually, EPD coatings are analyzed by means of electron microscopy,
mechanical tests, or functional tests, such as contact angle or corro-
sion resistance measurements, depending on their applications. Less
commonly EPD coatings are studied by Electrochemical Impedance
Spectroscopy (EIS) measurements, a technique that is preferably used
to study metal/solution interface, oxide films and surface treatments,
as well as corrosion behavior of organic paints on metals.
Generally EIS is an outstanding technique for studying the in-
teraction between electrolyte and electrode,4–7 and therefore it is the
proper method for investigating the potential of coatings as batteries,8,9
supercapacitors,10,11 sensors,12,13 or thermal barrier coatings.14–16 To
the best of the authors’ knowledge, EIS has not been used yet to in-
vestigate the morphological properties of EPD deposits, although this
method should potentially allow to obtain qualitative information on
thickness, porosity, and electrochemical properties simultaneously.
EIS has some remarkable advantages: (i) its theoretical and practi-
cal background has been developed since some decades, and therefore
adequately validated; (ii) it can be applied regardless of chemistry, de-
position technique and thickness; (iii) it is particularly useful when
the analyzing coating contains open pores or vertical cracks; (iv) it is
characterized by a rapid acquisition of data, repeatability, and accu-
racy; (v) potentially it can detect sub-critical damages and associated
failure mechanisms.
In general, when EIS is used for studying a coating, electric prop-
erties of materials and interfaces are considered, and therefore elec-
trolyte conductivity and micro-structural features of coatings, includ-
ing porosity and damage through which electrolyte can penetrate, are
examined. The analyzed system composed by electrolyte, electrolyte-
coating interface, coating, also multi-layered, is represented by an
equivalent electrical circuit having a similar electrical behavior of the
z
E-mail: federica.dericcardis@enea.it
physical analyzed system. In order to recognize the system features,
the complex impedance of the equivalent circuit has to be studied. It
is worthwhile to consider that often it is difficult to understand the
effective relationship between the measured complex impedance and
the interface reaction occurring on a coating. For this reason EIS must
be used with great care. Moreover, it should be stressed that EIS, as
a complementary technique, can supply information that needs other
methods to explain or confirm the supposed interfacial processes or
to obtain physical quantitative data.
The principal purpose of this article is to examine the possibility
of using EIS as a non-destructive technique suitable for evaluating
some morphological properties of EPD coatings, such as thickness
and porosity. At this aim, three classes of samples with different mor-
phological characteristics were examined. The first class had different
thickness and equal morphological features on surface, the second
kind of coatings was characterized by a notable porosity, and the third
kind had submicron roughness as characterizing parameter. All these
classes of coatings contain poly-ether-ether-ketone (PEEK), so that
the interface reactions with electrolyte are similar and therefore they
are not considered at the aim of this work.
Beyond classical models proposed by literature to simulate organic
or porous coatings,4–7 other models with a better fit of experimental
data were used. Although a complete interpretation of these models
is hard and the discussion on their validity is certainly open, the
benefits of EIS in a rapid investigation of EPD coatings, especially in
morphological terms, are undeniable.
Experimental
EPD coatings were obtained by using different suspensions and dif-
ferent deposition conditions. Coatings containing only polyetherether-
ketone (PEEK) powder and PEEK and alumina powders were de-
posited on stainless steel and carbon paper respectively, as described
in Refs. 17 and 18. Coatings based on PEEK and polytetrafluoroethy-
lene (PTFE) were deposited on silicon substrate following the pro-
cedure reported in Ref. 19. After deposition, thermal treatment was
performed in order to densify the coatings based on PEEK. The con-
dition of deposition process and of thermal treatment are reported in
Table I.
EIS investigation was performed at room temperature in a three
electrode cell, where the EPD coating deposited on its respective
substrate was used as working electrode, with an Ag/AgCl as reference
electrode and a platinum wire as counter electrode. Electrolyte was

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 D3072 Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015)

Table I. Parameters used for deposition and thermal treatment of investigated samples.

(a) PEEK
Deposition parameters

Suspension Applied Deposition Thermal treatment Deposited mass

No. composition voltage (V) time (s) conditions density (mg/cm2 )

P1 2.4 g/l PEEK powder 15 60 10 min @320◦ C 0.21

P2 in acetone 30 60 1.26
P3 50 60 2.11
P4 75 60 3.30
(b) PEEK-Al2 O3
Deposition parameters

Suspension Applied Deposition Thermal treatment Thickness Porosity SSA

No. composition voltage (V) time (s) conditions (μm) (%) (m2 /g)
PA1 2.5 wt% of power in ethanol 30 60 60 min @ 340◦ C 14 29 53
PA2 PEEK:Al2 O3 = 1:1 50 60 18 31 66
PA3 30 300 65 49 567
PA4 50 300 95 57 613
(c) PEEK-PTFE
Deposition parameters

Suspension Applied Deposition Thermal treatment Roughness

No. composition voltage (V) time (s) conditions (nm)

PP1 1.2 wt% of power in ethanol 100 60 10 min @300◦ C 225

PEEK:PTFE = 1:4
PP2 1.2 wt% of power in ethanol 100 60 360
PEEK:PTFE = 1:1
PP3 1.2 wt% of power in ethanol 100 60 550
PEEK:PTFE = 4:1

supplied by a 35 g/l NaCl aqueous solution and coating exposed area
was about 0.8 cm2 . The three-electrode cell was connected to a 2273
FRA (Princeton Applied Research) measurement system in remote
control. A sinusoidal voltage perturbation of 10 mV in amplitude
around the open circuit potential (OCP) with a frequency range from
10 mHz to 1 MHz was input to the system. The system response was
recorded both as Bode and as Nyquist plots and data processing was
performed by using Zsimpwin software (Ametek). Some comments
on the equivalent circuits used to fit the acquired EIS spectra are
reported in Supplemental Material section.
For morphological investigations, a scanning electron microscope
(Merlin, ZEISS) and an atomic force microscope (Nanoscope IIIA,
Digital Instruments) were used. Roughness measurements were per-
formed by AFM on several images of 250 μm2 areas, with an ex-
perimental error estimated equal to 10%. Specific surface area and
pore volume were measured by BET method (Autosorb iQ, Quan-
tachrome) using nitrogen as adsorbate. Finally, the macroporosity of
samples containing PEEK and Alumina was evaluated by pycnometer
method.
Results and Discussion
EIS on stainless steel substrate.— As first measurement, a system
constituted by a thin oxide layer on stainless steel (SS) was analyzed
by EIS. The oxide layer, amber colored, was obtained by a thermal
treatment of SS substrates at 320◦ in air for 10 minutes. This material
was chosen for a double aim: firstly, because the thermal treatment
produced a simple system formed by a coating strictly adherent to
substrate; second, because stainless steel was used as substrate for the
EPD PEEK coatings investigated by EIS, as described in this work. In
such way, an evaluation of the role of the oxide layer on EIS spectra
can be deduced.
The thickness of the oxide film grown on stainless was evaluated of
about 10 nm by optical measurements. For the oxide film on stainless
steel, the equivalent circuit containing two RC loop well fitted the
relative EIS spectrum. In Figs. 1a and 1b the corresponding Nyquist
and Bode plots are reported. With this example, EIS demonstrated to
be sensible also to a thin layer applied on a substrate.
Correlation between thickness and Rcoat .— The usual equivalent
circuit adopted for describing a porous organic coating is reported in
Fig. 2. The first RC loop is generally related to macroscopic proper-
ties of the coating surface, including defects. Resistance is referred
to coating thickness (Rcoat ) whereas capacitance (Ccoat ) is relative to
coating and porosity. The second RC loop is related to electrochem-
istry on coating defects, and is composed by charge transfer resistance
(Rct ) and double layer capacitance (Cdl ).
An ideally capacitive impedance should be observed on atomi-
cally and geometrically uniform electrodes. On polycrystalline solid
electrodes, even if smooth, impedance is not purely capacitive, but a
double layer capacitance depending on frequency is observed. Other
features such as porosity, pore shape and other defects can also con-
tribute to the non-uniform distribution in the current density. For these
reasons, often capacitance does not have an ideal behavior, and a con-
stant phase element (CPE) instead of capacitor is used in order to
represent the deviation of the real capacitance from ideality.4–7
The suitability of this model was verified for EPD PEEK coat-
ings deposited on stainless steel. Different values of voltage (from
15 to 75 V) were applied to a suspension of PEEK in acetone for
a deposition time equal to 60 s (Table Ia). Therefore samples with
different deposited mass were obtained. After deposition, all PEEK
coatings were simultaneously treated in air at 320◦ C for 10 min-
utes. The morphology of the sample surface is typically that shown
in Fig. 3.
EIS spectra recorded on this kind of samples are shown in Fig. 4
and the parameter values of the corresponding equivalent circuits are
reported in Table II. In this sample series, the distinguish element
was the increasing thickness, that is correlated to Rcoat . In Fig. 5
a linear relationship between Rcoat values and the deposited mass
density is shown, demonstrating the effectiveness of EIS technique

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 Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015) D3073

12000 -100

-90
10000
-80
8000
-70

Phase of Z (deg)
(ohm)

6000 -60

|Z| (ohm)
-50
4000
-40

2000 -30

-20
0
-10
-2000
0
0,01 0,1 1 10 100 1000 10000 100000 1000000

(ohm) Frequency (Hz)

(a) (b)

Figure 1. Nyquist (a) and Bode (b) plots acquired on oxidised stainless steel, simulated by the equivalent circuit reported in inset.

in discriminating samples with different deposited mass density and

therefore different thickness.

Correlation between porosity and Cdl .— A second class of coat-

ings was considered in order to investigate the relationship between
porosity and equivalent circuit parameters. In this case composite coat-
ings containing PEEK and Alumina powder were prepared, applying
a voltage of 30 and 50 V to an ethanol solution with a PEEK/Alumina
weight ratio equal to 1 for a deposition time equal to 60 and 300 s. The
deposited coatings were thermally treated at 340◦ C for 1 hour in order
to make them more compact. Since the melting point of PEEK is about
at 340◦ C, PEEK powder resulted almost melted and produced a cer-
tain porosity both on surface and inside the thickness. In Fig. 6 SEM
micrographs referring to surface and cross section of PEEK-Alumina
composite coatings are reported. The porosity, being at microscopic
scale, was measured by pycnometer method immersing the samples
in water.
The equivalent circuit better fitting the EIS spectra acquired on this
class of samples is again that reported in Fig. 2 with CPE1 instead of
Ccoat . The corresponding parameter values are reported in Table III. Figure 3. SEM image (at different magnification) of a typical surface of a
Bode plots recorded during EIS measurements showed a plateau in PEEK coating deposited by EPD on stainless steel and thermally treated at
real impedance (Fig. 7a) for the frequency range 0.1 Hz - 10 MHz, 320◦ C.
attributed to coating resistance, and a peak at high frequency in the
phase plot (Fig. 7b), corresponding to porosity.
The resistance values corresponding to plateau, which in turn is -10000

associated to Rcoat , were linearly related to thickness of composite

coating, as expected and as demonstrated by graph reported in Fig. 8.
-8000

-6000
-Z '' (ohm)

-4000

-2000

0 5000 10000 15000 20000

Z ' (ohm)

Figure 2. Equivalent circuit for a porous organic coating with ideal Figure 4. EIS spectra acquired on PEEK coatings: P1 (circles), P2 (dia-
capacitance. monds), P3 (squares), and P4 (triangles).

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 D3074 Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015)

Table II. Values of the equivalent circuit fitting EIS spectra acquired on PEEK coatings.

No. Rcoat () CPE1 ((F · s)−n ) n Rct () CPE2 ((F · s)−n ) n χ2
P1 1.21 E3 4.72 E-5 0.49 7.69 E3 1.22 E-4 0.74 2.3 E-2
P2 9.66 E3 1.06 E-6 0.56 7.68 E5 4.22 E-6 0.91 2.0 E-2
P3 1.99 E4 1.74 E-6 0.48 7.43 E4 7.60 E-5 0.73 6.8 E-3
P4 3.80 E4 1.45 E-6 0.90 7.97 E7 6.04 E-8 0.95 3.1 E-2

4
4,5x10

4
4,0x10

4
3,5x10

4
3,0x10

4
2,5x10
Rcoat(ohm )

4
2,0x10

4
1,5x10

4
1,0x10

3
5,0x10

0,0

0,0 0,5 1,0 1,5 2,0 2,5 3,0 3,5

2
Deposited mass density (mg/cm )
Figure 6. SEM image of surface and cross section (inset) of a typical PEEK-
Alumina composite coating deposited by EPD and thermally treated at 340◦ C.
Figure 5. Linear relationship between Rcoat and deposited mass density for
PEEK coatings.
Table III. Values of the equivalent circuit parameters for PEEK-
Alumina composite coatings.
An exponential relationship between the measured porosity and the
Cdl values was recognized and a similar of Cdl dependence from thick- No. Rcoat () CPE1 ((F · s)−n ) n Rct () Cdl (F) χ2
ness was obtained (Fig. 9). This result indicates an abrupt increase of PA1 8.40 E3 6.09 E-7 0.32 5.63 E5 2.04 E-10 2.1 E-2
double layer capacitance at the highest value of porosity and thick- PA2 9.48 E3 6.33 E-5 0.12 3.06 E7 4.60 E-10 4.2 E-2
ness, probably due to an additive effect of increased exposed surface PA3 8.63 E4 7.36 E-11 0.98 8.40 E3 8.84 E-8 1.0 E-2
of pores and significant mass participating to electrochemical pro- PA4 1.56 E5 1.18 E-10 0.89 2.86 E9 4.47 E-6 3.3 E-3
cess induced by EIS experiment. As a proof supporting this hypoth-
esis, specific surface area (SSA) measurements were performed by
BET method. The shape of the isotherm adsorption-desorption curves This outcome contributes to justify the amplified SSA at high thick-
(Fig. 10) showed a behavior recognizable as the V type of IUPAC ness values and therefore the sudden rise of Cdl (Table III).
classification,20 meaning that mesopores were present. Moreover, the Also in this case, EIS measurement on porous EPD coatings were
hysteresis loop indicated that porosity was irregularly distributed in suitable to give qualitative information on coating quality, in terms of
thickness, and probably some crevices were formed connecting pores. trend of thickness and porosity as function of deposition parameters.

Figure 7. Bode plot of impedance modulus (a) and phase (b) recorded on PEEK-Alumina composite coatings deposited by EPD at different applied voltage for
different deposition time: PA1 (triangles), PA2 (squares), PA3 (circles), PA4 (diamonds).

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 Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015) D3075

5 3000
2x10
5
2x10
2500
5
1x10

Volume adsorbed (cm /g)

5 2000
1x10

3
5
1x10
Rcoat(ohm)

1500
4
8x10

6x10
4 1000

4
4x10
500
4
2x10

0 0

0 20 40 60 80 100 0,0 0,2 0,4 0,6 0,8 1,0

Thickness (micron) Relative pressure (P/P0)

Figure 8. Linear relationship between thickness and values of Rcoat for PEEK- Figure 10. Typical isotherm adsorption (circles) – desorption (squares) curves
Alumina composite coatings. acquired on PEEK-Alumina EPD coatings.

5
1,4x10
Correlation between roughness and n.— To verify the suitability of
EIS technique in investigating EPD coatings characterized by a quasi- 5
1,2x10
null porosity and a roughness at submicron scale, samples containing
PEEK and PTFE were expressly prepared. A suspension containing 5
1,0x10
the two polymer powders in different weight ratio dispersed in ethanol
was used, as reported in Table Ic. The coatings were obtained by ap-
Z Im (ohm)

4
8,0x10
plying 100 V for 60 s to a silicon substrate used as working electrode.
After deposition, the samples were thermally treated in air at 300◦ C 4
6,0x10
for 10 minutes.
The recorded EIS spectra were reported in Fig. 11 and were in- 4
4,0x10
terpolated by using an equivalent circuit with a Warburg impedance
in series with Rcoat (see Supplemental Material). The corresponding 4
2,0x10
parameter values are reported in Table IV.
A relationship was found between n of CPE and surface roughness
0,0
evaluated qualitatively by SEM and quantitatively by means of AFM
measurements. Small rounded features (with a mean height of 65 nm) 0,0 5,0x10
4
1,0x10
5
1,5x10
5

alternated to flat zones like terraces (meanly of 100 nm in height) are Z Re (ohm)
visible on the surface of all PEEK-PTFE coatings (Figs. 12,13). The
roughness, ranging from 225 to 550 nm, was determined by the more Figure 11. Nyquist plots acquired on PEEK-PTFE coatings: PP1 (closed cir-
or less extended parts containing the rounded particulars and the flat cles), PP2 (triangles), PP3 (squares).

-5 -5
1x10 1x10

-6 -6
1x10 1x10

-7 -7
1x10 1x10
Cdl(F)
Cdl(F)

-8 -8
1x10 1x10

-9 -9
1x10 1x10

-10 -10
1x10 1x10

20 30 40 50 60 70 0 20 40 60 80 100
Porosity (%) Thickness (micron)
(a) (b)

Figure 9. Exponential relationship between porosity (a) and thickness (b) and Cdl value for PEEK-Alumina composite coatings.

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 D3076 Journal of The Electrochemical Society, 162 (11) D3071-D3076 (2015)

Figure 12. SEM images of the surface of PEEK-PTFE coatings: PP1 (left), PP2 (middle), and PP3 (right).

Table IV. Values of the equivalent circuit parameters for PEEK- zones. As predicted by theory, n is inversely correlated with the surface
PTFE composite coatings. roughness, as shown in Fig. 14. Also in this case, EIS demonstrated
to be a technique applicable to morphological investigation of EPD
No. Rcoat () CPE ((F · s)−n ) n W ((F · s)−n ) χ2 coatings characterized by a submicron roughness.
PP1 2.56 E4 5.84 E-7 0.81 1.48 E-5 3.2 E-2
PP2 1.60 E3 1.97 E-6 0.76 2.11 E-5 5.5 E-2 Conclusions
PP3 4.83 E3 6.82 E-6 0.59 2.7 E-5 1.0 E-2
Although Electrochemical impedance spectroscopy is the most dif-
fuse and reliable technique used to study corrosion and/or capacitive
properties of coatings, in this work EIS was used to investigate EPD
coatings from a morphological point of view. At this aim, three classes
of EPD coatings were used. Each class of coatings was characterized
by a different morphological feature, such as thickness, porosity, and
roughness. Suitable equivalent circuits were defined and a relation-
ship between equivalent circuit parameters and physical parameters of
coatings was established. Although EIS cannot give quantitative eval-
uation of morphological parameters of EPD coatings, this technique
demonstrated its potential as non-destructive and quick method to ob-
tain qualitative information, particularly useful when a comparison be-
tween samples with different morphological characteristics is sought.

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